U.S. patent application number 17/176480 was filed with the patent office on 2021-06-03 for translucent smokeless tobacco product.
The applicant listed for this patent is R.J. Reynolds Tobacco Company. Invention is credited to Darrell Holton, JR..
Application Number | 20210161196 17/176480 |
Document ID | / |
Family ID | 1000005404480 |
Filed Date | 2021-06-03 |
United States Patent
Application |
20210161196 |
Kind Code |
A1 |
Holton, JR.; Darrell |
June 3, 2021 |
TRANSLUCENT SMOKELESS TOBACCO PRODUCT
Abstract
The invention provides a smokeless tobacco product comprising a
tobacco extract. In some embodiments, the smokeless tobacco product
is translucent. The invention further provides methods for making
and using the smokeless tobacco product. In certain embodiments,
the smokeless tobacco product comprises isomalt, maltitol syrup,
and a translucent tobacco extract prepared by ultrafiltration.
Inventors: |
Holton, JR.; Darrell;
(Clemmons, NC) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
R.J. Reynolds Tobacco Company |
Winston-Salem |
NC |
US |
|
|
Family ID: |
1000005404480 |
Appl. No.: |
17/176480 |
Filed: |
February 16, 2021 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
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15884888 |
Jan 31, 2018 |
10952461 |
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17176480 |
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14789020 |
Jul 1, 2015 |
9901113 |
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15884888 |
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13240525 |
Sep 22, 2011 |
9084439 |
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14789020 |
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Current U.S.
Class: |
1/1 |
Current CPC
Class: |
A24B 15/10 20130101;
A24B 15/30 20130101; A24B 15/24 20130101 |
International
Class: |
A24B 15/24 20060101
A24B015/24; A24B 15/10 20060101 A24B015/10; A24B 15/30 20060101
A24B015/30 |
Claims
1. A smokeless tobacco product comprising: a. a tobacco extract in
an amount of at least about 3% by weight; b. a sugar substitute in
an amount of at least about 80% by weight; and c. a sugar alcohol
syrup, wherein the smokeless tobacco product is translucent.
2. The smokeless tobacco product of claim 1, wherein the sugar
substitute is a non-hygroscopic sugar alcohol capable of forming a
glassy matrix.
3. The smokeless tobacco product of claim 1, wherein the sugar
substitute is isomalt.
4. The smokeless tobacco product of claim 1, wherein the sugar
substitute is present in an amount of at least about 85% by
weight.
5. The smokeless tobacco product of claim 1, wherein the sugar
substitute is present in an amount of at least about 90% by
weight.
6. The smokeless tobacco product of claim 1, wherein the sugar
alcohol syrup is maltitol syrup.
7. The smokeless tobacco product of claim 1, wherein the tobacco
extract is an ultrafiltered tobacco extract characterized as
translucent or transparent.
8. The smokeless tobacco product of claim 1, wherein the tobacco
extract is a heat-treated tobacco extract that has been treated
prior to inclusion in the smokeless tobacco product by heating the
tobacco extract in an aqueous solution comprising L-lysine,
L-cysteine, asparaginase, or hydrogen peroxide.
9. The smokeless tobacco product of claim 8, wherein the aqueous
solution further comprises NaOH.
10. The smokeless tobacco product of claim 1, wherein the tobacco
extract is a heat-treated tobacco extract that has been treated
prior to inclusion in the smokeless tobacco product by heating the
tobacco extract in an aqueous solution comprising L-lysine and
NaOH.
11. The smokeless tobacco product of claim 1, wherein the tobacco
extract consists of compounds having a molecular weight of less
than about 50,000 Da.
12. The smokeless tobacco product of claim 10, wherein the tobacco
extract consists of compounds having a molecular weight of less
than about 5,000 Da.
13. The smokeless tobacco product of claim 1, further comprising
one or more flavorants.
14. The smokeless tobacco product of claim 12, wherein the amount
of flavorant is from about 0.1 to about 0.5 percent by weight of
the smokeless tobacco product.
15. The smokeless tobacco product of claim 13, wherein the
flavorant is vanillin or mint flavor.
16. The smokeless tobacco product of claim 1, further comprising at
least one sweetener.
17. The smokeless tobacco product of claim 15, wherein the at least
one sweetener comprises sucralose.
18. The smokeless tobacco product of claim 1, further comprising
NaCl.
19. The smokeless tobacco product of claim 17, wherein the amount
of NaCl is from about 0.5 to about 1 percent by weight of the
smokeless tobacco product.
20. (canceled)
21. A method of preparing a translucent smokeless tobacco product,
comprising: (i) mixing a translucent or transparent tobacco extract
with a non-hygroscopic sugar alcohol capable of forming a glassy
matrix in a melted state to form a mixture; and (ii) cooling the
mixture to room temperature to form a solid smokeless tobacco
product exhibiting translucency.
22.-32. (canceled)
Description
FIELD OF THE INVENTION
[0001] The present invention relates to products made or derived
from tobacco, or that otherwise incorporate tobacco, and are
intended for human consumption. In particular, the invention
relates to smokeless tobacco products containing ingredients or
components obtained or derived from plants of the Nicotiana
species.
BACKGROUND OF THE INVENTION
[0002] Cigarettes, cigars and pipes are popular smoking articles
that employ tobacco in various forms. Such smoking articles are
used by heating or burning tobacco, and aerosol (e.g., smoke) is
inhaled by the smoker. Tobacco also may be enjoyed in a so-called
"smokeless" form. Particularly popular smokeless tobacco products
are employed by inserting some form of processed tobacco or
tobacco-containing formulation into the mouth of the user. See for
example, the types of smokeless tobacco formulations, ingredients,
and processing methodologies set forth in U.S. Pat. No. 1,376,586
to Schwartz; U.S. Pat. No. 3,696,917 to Levi; U.S. Pat. No.
4,513,756 to Pittman et al.; U.S. Pat. No. 4,528,993 to Sensabaugh,
Jr. et al.; U.S. Pat. No. 4,624,269 to Story et al.; U.S. Pat. No.
4,991,599 to Tibbetts; U.S. Pat. No. 4,987,907 to Townsend; U.S.
Pat. No. 5,092,352 to Sprinkle, III et al.; U.S. Pat. No. 5,387,416
to White et al.; U.S. Pat. No. 6,668,839 to Williams; U.S. Pat. No.
6,834,654 to Williams; U.S. Pat. No. 6,953,040 to Atchley et al.;
U.S. Pat. No. 7,032,601 to Atchley et al.; and U.S. Pat. No.
7,694,686 to Atchley et al.; US Pat. Pub. Nos. 2004/0020503 to
Williams; 2005/0115580 to Quinter et al.; 2006/0191548 to
Strickland et al.; 2007/0062549 to Holton, Jr. et al.; 2007/0186941
to Holton, Jr. et al.; 2007/0186942 to Strickland et al.;
2008/0029110 to Dube et al.; 2008/0029116 to Robinson et al.;
2008/0173317 to Robinson et al.; 2008/0196730 to Engstrom et al.;
2008/0209586 to Neilsen et al.; 2008/0305216 to Crawford et al.;
2009/0065013 to Essen et al.; 2009/0293889 to Kumar et al.; and
2010/0291245 to Gao et al; PCT WO 04/095959 to Arnarp et al. and WO
2010/132444 A2 to Atchley; and U.S. patent application Ser. No.
12/638,394, filed Dec. 15, 2009, to Mua et al.; each of which is
incorporated herein by reference. Exemplary smokeless tobacco
products that have been marketed include those referred to as CAMEL
Snus, CAMEL Orbs, CAMEL Strips and CAMEL Sticks by R. J. Reynolds
Tobacco Company; GRIZZLY moist tobacco, KODIAK moist tobacco, LEVI
GARRETT loose tobacco and TAYLOR'S PRIDE loose tobacco by American
Snuff Company, LLC; KAYAK moist snuff and CHATTANOOGA CHEW chewing
tobacco by Swisher International, Inc.; REDMAN chewing tobacco by
Pinkerton Tobacco Co. LP; COPENHAGEN moist tobacco, COPENHAGEN
Pouches, SKOAL Bandits, SKOAL Pouches, RED SEAL long cut and REVEL
Mint Tobacco Packs by U.S. Smokeless Tobacco Company; and MARLBORO
Snus and Taboka by Philip Morris USA.
[0003] It would be desirable to provide an enjoyable form of a
tobacco product, such as a smokeless tobacco product, and to
provide processes for preparing tobacco-containing compositions
suitable for use in smokeless tobacco products.
SUMMARY OF THE INVENTION
[0004] The present invention provides a smokeless tobacco product
comprising tobacco or a derivative thereof obtained from plants of
the Nicotiana species. The products of the invention are
dissolvable compositions adapted for oral consumption and exhibit a
level of translucency despite containing a tobacco or
tobacco-derived material. In certain embodiments, the products
comprise a tobacco extract that can be characterized as translucent
or transparent.
[0005] In one aspect of the present invention, the invention
provides a smokeless tobacco product comprising: a tobacco extract
in an amount of at least about 3% by weight; a sugar substitute in
an amount of at least about 80% by weight; and a sugar alcohol
syrup, wherein the smokeless tobacco product is translucent. The
amount and type of the sugar substitute can vary. In certain
embodiments, the sugar substitute is a non-hygroscopic sugar
alcohol capable of forming a glassy matrix. For example, in some
embodiments, the sugar substitute is isomalt. In certain
embodiments, the sugar substitute is present in an amount of at
least about 85% by weight or at least about 90% by weight. In some
embodiments, the sugar alcohol syrup is maltitol syrup.
[0006] In certain embodiments, the tobacco extract is an
ultrafiltered tobacco extract that can be characterized as
translucent or transparent. The extract can be, in some
embodiments, a heat-treated tobacco extract that has been treated
prior to inclusion in the smokeless tobacco product by heating the
tobacco extract in an aqueous solution comprising L-lysine,
L-cysteine, asparaginase, or hydrogen peroxide. The aqueous
solution can comprise additional additives; for example, in some
embodiments, the aqueous solution further comprises NaOH. In one
exemplary embodiment, a smokeless tobacco product is provided,
wherein the tobacco extract is a heat-treated tobacco extract that
has been treated prior to inclusion in the smokeless tobacco
product by heating the tobacco extract in an aqueous solution
comprising L-lysine and NaOH.
[0007] In some embodiments, the smokeless tobacco product can be
characterized by the content of high molecular weight compounds. In
one embodiment, the tobacco extract consists of compounds having a
molecular weight of less than about 50,000 Da. In another
embodiment, the tobacco extract consists of compounds having a
molecular weight of less than about 5,000 Da.
[0008] The smokeless tobacco product can further comprise any one
or more additional additives. For example, in some embodiments, the
smokeless tobacco product comprises one or more flavorants. The
amount of flavorant can vary; for example, flavorant can be
included in an amount of from about 0.1 to about 0.5 percent by
weight of the smokeless tobacco product. In certain embodiments, it
can be included in an amount up to about 2% or up to about 5% by
weight of the smokeless tobacco product. The flavorant can be, in
certain embodiments, vanillin and/or mint flavor. In some
embodiments, the smokeless tobacco product further comprises at
least one sweetener. One exemplary sweetener that can be used
according to the invention is sucralose. In some embodiments, the
smokeless tobacco product further comprises NaCl. The NaCl can be
present in varying amounts; for example, in some embodiments, the
amount of NaCl is from about 0.5 to about 1 percent by weight of
the smokeless tobacco product. In certain embodiments, the amount
of NaCl can be included in an amount of up to about 4% or up to
about 8% by weight of the smokeless tobacco product.
[0009] In another aspect of the present invention, the invention
provides a smokeless tobacco product comprising: a tobacco extract
consisting of components having a molecular weight of no more than
about 50,000 Da in an amount of at least about 3% by weight; a
non-hygroscopic sugar alcohol capable of forming a glassy matrix in
an amount of at least about 80% by weight; and a sugar alcohol
syrup in an amount sufficient to slow recrystallization of the
non-hygroscopic sugar alcohol, wherein the smokeless tobacco
product is translucent.
[0010] In a further aspect of the invention, the invention provides
a method of preparing a translucent smokeless tobacco product,
comprising: mixing a translucent or transparent tobacco extract
with a non-hygroscopic sugar alcohol capable of forming a glassy
matrix in a melted state to form a mixture; and cooling the mixture
to room temperature to form a solid smokeless tobacco product
exhibiting translucency. The translucent or transparent tobacco
extract can, in some embodiments, be treated prior to use in the
method. For example, the tobacco extract can be treated by size
exclusion chromatography, microfiltration, ultrafiltration,
nanofiltration, reverse osmosis, or a combination thereof to
produce the translucent or transparent tobacco extract. In certain
embodiments, the treatment removes components having a molecular
weight above about 50,000 Da. In some embodiments, the translucent
or transparent tobacco extract has been heat treated prior to use
in the method. For example, the tobacco extract can be heated in an
aqueous solution comprising L-lysine, L-cysteine, asparaginase, or
hydrogen peroxide. In some embodiments, the tobacco extract is
heated in such an aqueous solution, which can further comprise
NaOH. In certain embodiments, the heat treating step is conducted
at about 88.degree. C. Using a heat treated tobacco extract can, in
some embodiments, give a smokeless tobacco product having less than
about 500 ppb acrylamide.
[0011] In some embodiments, the method of preparing a translucent
smokeless tobacco product comprises heating the non-hygroscopic
sugar alcohol to a temperature above the hard crack stage in the
absence of the tobacco extract and mixing the tobacco extract into
the non-hygroscopic sugar alcohol at a temperature below the hard
crack stage. The temperatures can vary; however, in certain
embodiments, the hard crack stage is about 145.degree. C. to about
155.degree. C. and the non-hygroscopic sugar alcohol is heated at a
temperature between the hard crack stage and about 171.degree. C.
In some embodiments, the method further comprises introducing the
mixture into molds to create individual product units prior to the
cooling step.
[0012] In another aspect of the invention, the invention provides a
method of preparing a translucent or transparent extract for
incorporating into a smokeless tobacco product, comprising:
extracting a tobacco material with an aqueous solvent to form an
aqueous tobacco extract; ultrafiltering the aqueous tobacco extract
to remove components having a molecular weight above about 50,000
Da to form a translucent or transparent tobacco extract; and heat
treating the tobacco extract prior to or after the ultrafiltering
step by heating the extract in an aqueous solution comprising
L-lysine, L-cysteine, asparaginase, or hydrogen peroxide. In
certain embodiments, the ultrafiltering step comprises passing the
aqueous tobacco extract through multiple ultrafiltration
membranes.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0013] The present invention now will be described more fully
hereinafter. This invention may, however, be embodied in many
different forms and should not be construed as limited to the
embodiments set forth herein; rather, these embodiments are
provided so that this disclosure will be thorough and complete, and
will fully convey the scope of the invention to those skilled in
the art. As used in this specification and the claims, the singular
forms "a," "an," and "the" include plural referents unless the
context clearly dictates otherwise. Reference to "dry weight
percent" or "dry weight basis" refers to weight on the basis of dry
ingredients (i.e., all ingredients except water).
[0014] The present invention relates to smokeless tobacco products
adapted for oral consumption that contain tobacco or a
tobacco-derived material and that exhibit translucence or
transparency, such as a product in the form of a translucent
lozenge. The invention provides a process for preparing a tobacco
material that can impart tobacco flavor to the product without
reducing clarity of the product to the point of opacity, and a
process for preparing a translucent product using such a tobacco
material.
[0015] The selection of the plant from the Nicotiana species
utilized in the products and processes of the invention can vary;
and in particular, the types of tobacco or tobaccos may vary. The
type of tobacco used as both the source of tobacco stalks and as
the carrier for the syrup of the invention can vary. Tobaccos that
can be employed include flue-cured or Virginia (e.g., K326),
burley, sun-cured (e.g., Indian Kurnool and Oriental tobaccos,
including Katerini, Prelip, Komotini, Xanthi and Yambol tobaccos),
Maryland, dark, dark-fired, dark air cured (e.g., Passanda, Cubano,
Jatin and Bezuki tobaccos), light air cured (e.g., North Wisconsin
and Galpao tobaccos), Indian air cured, Red Russian and Rustica
tobaccos, as well as various other rare or specialty tobaccos.
Descriptions of various types of tobaccos, growing practices and
harvesting practices are set forth in Tobacco Production, Chemistry
and Technology, Davis et al. (Eds.) (1999), which is incorporated
herein by reference. Various representative types of plants from
the Nicotiana species are set forth in Goodspeed, The Genus
Nicotiana, (Chonica Botanica) (1954); U.S. Pat. No. 4,660,577 to
Sensabaugh, Jr. et al.; U.S. Pat. No. 5,387,416 to White et al.;
U.S. Pat. No. 7,025,066 to Lawson et al.; and U.S. Pat. No.
7,798,153 to Lawrence, Jr.; and US Patent Appl. Pub. No.
2008/0245377 to Marshall et al.; each of which is incorporated
herein by reference.
[0016] Exemplary Nicotiana species include N. tabacum, N. rustica,
N. alata, N. arentsii, N. excelsior, N. forgetiana, N. glauca, N.
glutinosa, N. gossei, N. kawakamii, N. knightiana, N. langsdorffi,
N. otophora, N. setchelli, N. sylvestris, N. tomentosa, N.
tomentosiformis, N. undulata, N. x sanderae, N. africana, N.
amplexicaulis, N. benavidesii, N. bonariensis, N. debneyi, N.
longiflora, N. maritina, N. megalosiphon, N. occidentalis, N.
paniculata, N. plumbaginifolia, N. raimondii, N. rosulata, N.
simulans, N. stocktonii, N. suaveolens, N. umbratica, N. velutina,
N. wigandioides, N. acaulis, N. acuminata, N. attenuata, N.
benthamiana, N. cavicola, N. clevelandii, N. cordifolia, N.
corymbosa, N. fragrans, N. goodspeedii, N. linearis, N. miersii, N.
nudicaulis, N. obtusifolia, N. occidentalis subsp. hersperis, N.
pauciflora, N. petunioides, N. quadrivalvis, N. repanda, N.
rotundifolia, N. solanifolia and N. spegazzinii.
[0017] Nicotiana species can be derived using genetic modification
or crossbreeding techniques (e.g., tobacco plants can be
genetically engineered or crossbred to increase or decrease
production of components, characteristics or attributes). See, for
example, the types of genetic modifications of plants set forth in
U.S. Pat. No. 5,539,093 to Fitzmaurice et al.; U.S. Pat. No.
5,668,295 to Wahab et al.; U.S. Pat. No. 5,705,624 to Fitzmaurice
et al.; U.S. Pat. No. 5,844,119 to Weigl; U.S. Pat. No. 6,730,832
to Dominguez et al.; U.S. Pat. No. 7,173,170 to Liu et al.; U.S.
Pat. No. 7,208,659 to Colliver et al. and U.S. Pat. No. 7,230,160
to Benning et al.; US Patent Appl. Pub. No. 2006/0236434 to
Conkling et al.; and 2008/0209586 to Nielsen et al., which are all
incorporated herein by reference.
[0018] For the preparation of smokeless tobacco products, it is
typical for harvested plants of the Nicotiana species to be
subjected to a curing process. Descriptions of various types of
curing processes for various types of tobaccos are set forth in
Tobacco Production, Chemistry and Technology, Davis et al. (Eds.)
(1999). Exemplary techniques and conditions for curing flue-cured
tobacco are set forth in Nestor et al., Beitrage Tabakforsch. Int.,
20, 467-475 (2003) and U.S. Pat. No. 6,895,974 to Peele, which are
incorporated herein by reference. Representative techniques and
conditions for air curing tobacco are set forth in Roton et al.,
Beitrage Tabakforsch. Int., 21, 305-320 (2005) and Staaf et al.,
Beitrage Tabakforsch. Int., 21, 321-330 (2005), which are
incorporated herein by reference. Certain types of tobaccos can be
subjected to alternative types of curing processes, such as fire
curing or sun curing. Typically, harvested tobaccos that are cured
are then aged.
[0019] At least a portion of the plant of the Nicotiana species
(e.g., at least a portion of the tobacco portion) can be employed
in an immature form. That is, the plant, or at least one portion of
that plant, can be harvested before reaching a stage normally
regarded as ripe or mature. As such, for example, tobacco can be
harvested when the tobacco plant is at the point of a sprout, is
commencing leaf formation, is commencing flowering, or the like. At
least a portion of the plant of the Nicotiana species (e.g., at
least a portion of the tobacco portion) can be employed in a mature
form. That is, the plant, or at least one portion of that plant,
can be harvested when that plant (or plant portion) reaches a point
that is traditionally viewed as being ripe, over-ripe or mature. As
such, for example, through the use of tobacco harvesting techniques
conventionally employed by farmers, Oriental tobacco plants can be
harvested, burley tobacco plants can be harvested, or Virginia
tobacco leaves can be harvested or primed by stalk position.
[0020] The Nicotiana species can be selected for the content of
various compounds that are present therein. For example, plants can
be selected on the basis that those plants produce relatively high
quantities of one or more of the compounds desired to be isolated
therefrom. In certain embodiments, plants of the Nicotiana species
(e.g., Galpao commun tobacco) are specifically grown for their
abundance of leaf surface compounds. Tobacco plants can be grown in
greenhouses, growth chambers, or outdoors in fields, or grown
hydroponically.
[0021] Various parts or portions of the plant of the Nicotiana
species can be employed. For example, virtually all of the plant
(e.g., the whole plant) can be harvested, and employed as such.
Alternatively, various parts or pieces of the plant can be
harvested or separated for further use after harvest. For example,
the flower, leaves, stem, stalk, roots, seeds, and various
combinations thereof, can be isolated for further use or
treatment.
[0022] The post-harvest processing of the plant or portion thereof
can vary. After harvest, the plant, or portion thereof, can be used
in a green form (e.g., the plant or portion thereof can be used
without being subjected to any curing process). For example, the
plant or portion thereof can be used without being subjected to
significant storage, handling or processing conditions. In certain
situations, it is advantageous for the plant or portion thereof be
used virtually immediately after harvest. Alternatively, for
example, a plant or portion thereof in green form can be
refrigerated or frozen for later use, freeze dried, subjected to
irradiation, yellowed, dried, cured (e.g., using air drying
techniques or techniques that employ application of heat), heated
or cooked (e.g., roasted, fried or boiled), or otherwise subjected
to storage or treatment for later use.
[0023] The harvested plant or portion thereof can be physically
processed. The plant or portion thereof can be separated into
individual parts or pieces (e.g., the leaves can be removed from
the stems, and/or the stems and leaves can be removed from the
stalk). The harvested plant or individual parts or pieces can be
further subdivided into parts or pieces (e.g., the leaves can be
shredded, cut, comminuted, pulverized, milled or ground into pieces
or parts that can be characterized as filler-type pieces, granules,
particulates or fine powders). The plant, or parts thereof, can be
subjected to external forces or pressure (e.g., by being pressed or
subjected to roll treatment). When carrying out such processing
conditions, the plant or portion thereof can have a moisture
content that approximates its natural moisture content (e.g., its
moisture content immediately upon harvest), a moisture content
achieved by adding moisture to the plant or portion thereof, or a
moisture content that results from the drying of the plant or
portion thereof. For example, powdered, pulverized, ground or
milled pieces of plants or portions thereof can have moisture
contents of less than about 25 weight percent, often less than
about 20 weight percent, and frequently less than about 15 weight
percent.
[0024] The plant of the Nicotiana species or portions thereof can
be subjected to other types of processing conditions. For example,
components can be separated from one another, or otherwise
fractionated into chemical classes or mixtures of individual
compounds. Typical separation processes can include one or more
process steps (e.g., solvent extraction using polar solvents,
organic solvents, or supercritical fluids), chromatography,
distillation, filtration, recrystallization, and/or solvent-solvent
partitioning. Exemplary extraction and separation solvents or
carriers include water, alcohols (e.g., methanol or ethanol),
hydrocarbons (e.g., heptane and hexane), diethyl ether methylene
chloride and supercritical carbon dioxide. Exemplary techniques
useful for extracting components from Nicotiana species are
described in U.S. Pat. No. 4,144,895 to Fiore; U.S. Pat. No.
4,150,677 to Osborne, Jr. et al.; U.S. Pat. No. 4,267,847 to Reid;
U.S. Pat. No. 4,289,147 to Wildman et al.; U.S. Pat. No. 4,351,346
to Brummer et al.; U.S. Pat. No. 4,359,059 to Brummer et al.; U.S.
Pat. No. 4,506,682 to Muller; U.S. Pat. No. 4,589,428 to Keritsis;
U.S. Pat. No. 4,605,016 to Soga et al.; U.S. Pat. No. 4,716,911 to
Poulose et al.; U.S. Pat. No. 4,727,889 to Niven, Jr. et al.; U.S.
Pat. No. 4,887,618 to Bernasek et al.; U.S. Pat. No. 4,941,484 to
Clapp et al.; U.S. Pat. No. 4,967,771 to Fagg et al.; U.S. Pat. No.
4,986,286 to Roberts et al.; U.S. Pat. No. 5,005,593 to Fagg et
al.; U.S. Pat. No. 5,018,540 to Grubbs et al.; U.S. Pat. No.
5,060,669 to White et al.; U.S. Pat. No. 5,065,775 to Fagg; U.S.
Pat. No. 5,074,319 to White et al.; U.S. Pat. No. 5,099,862 to
White et al.; U.S. Pat. No. 5,121,757 to White et al.; U.S. Pat.
No. 5,131,414 to Fagg; U.S. Pat. No. 5,131,415 to Munoz et al.;
U.S. Pat. No. 5,148,819 to Fagg; U.S. Pat. No. 5,197,494 to Kramer;
U.S. Pat. No. 5,230,354 to Smith et al.; U.S. Pat. No. 5,234,008 to
Fagg; U.S. Pat. No. 5,243,999 to Smith; U.S. Pat. No. 5,301,694 to
Raymond et al.; U.S. Pat. No. 5,318,050 to Gonzalez-Parra et al.;
U.S. Pat. No. 5,343,879 to Teague; U.S. Pat. No. 5,360,022 to
Newton; U.S. Pat. No. 5,435,325 to Clapp et al.; U.S. Pat. No.
5,445,169 to Brinkley et al.; U.S. Pat. No. 6,131,584 to
Lauterbach; U.S. Pat. No. 6,298,859 to Kierulff et al.; U.S. Pat.
No. 6,772,767 to Mua et al.; and U.S. Pat. No. 7,337,782 to
Thompson, all of which are incorporated herein by reference. See
also, the types of separation techniques set forth in Brandt et
al., LC-GC Europe, p. 2-5 (March, 2002) and Wellings, A Practical
Handbook of Preparative HPLC (2006), which are incorporated herein
by reference. In addition, the plant or portions thereof can be
subjected to the types of treatments set forth in Ishikawa et al.,
Chem. Pharm. Bull., 50, 501-507 (2002); Tienpont et al., Anal.
Bioanal. Chem., 373, 46-55 (2002); Ochiai, Gerstel Solutions
Worldwide, 6, 17-19 (2006); Coleman, III, et al., J. Sci. Food and
Agric., 84, 1223-1228 (2004); Coleman, III et al., J. Sci. Food and
Agric., 85, 2645-2654 (2005); Pawliszyn, ed., Applications of Solid
Phase Microextraction, RSC Chromatography Monographs, (Royal
Society of Chemistry, UK) (1999); Sahraoui et al., J. Chrom., 1210,
229-233 (2008); and U.S. Pat. No. 5,301,694 to Raymond et al.,
which are all incorporated herein by reference.
[0025] According to the present invention, the Nicotiana plant or
portion thereof is typically subjected to processing intended to
provide improved clarity of the tobacco material. In certain
embodiments, the tobacco material used in the products of the
invention is in the form of an extract, such as an aqueous extract
of a tobacco material. Improved clarity of a tobacco extract can be
obtained, for example, by removing high molecular weight components
from the tobacco extract. In certain embodiments, high molecular
weight components that are beneficially removed according to the
present invention include, but are not limited to, high molecular
weight Maillard browning polymers, proteins, polysaccharides,
certain pigments, and bacteria. Various methods can be used for
this purpose, including size exclusion chromatography,
microfiltration, ultrafiltration, nanofiltration, reverse osmosis,
and combinations thereof.
[0026] In one embodiment, ultrafiltration is used to remove high
molecular weight components in the tobacco material. The
ultrafiltration method is typically applied to a tobacco material
comprising a tobacco extract (e.g., an aqueous tobacco extract). In
ultrafiltration, the material to be filtered is brought into
contact with a semipermeable membrane. The membrane can be of any
type, such as plate-and-frame (having a stack of membranes and
support plates), spiral-wound (having consecutive layers of
membrane and support material rolled up around a tube), tubular
(having a membrane-defined core through which the feed flows and an
outer, tubular housing where permeate is collected), or hollow
fiber (having several small diameter tubes or fibers wherein the
permeate is collected in the cartridge area surrounding the
fibers). The membrane can be constructed of any material. For
example, polysulfone, polyethersulfone, polypropylene,
polyvinylidenefluoride, and cellulose acetate membranes are
commonly used, although other materials can be used without
departing from the invention described herein.
[0027] Ultrafiltration membranes are available in a wide range of
pore sizes (typically ranging from about 0.1 to about 0.001
microns). Membranes are more typically described by their molecular
weight cutoffs. Ultrafiltration membranes are commonly classified
as membranes with number average molecular weight cutoffs of from
about 10.sup.3 Da to about 10.sup.5 Da. In practice, compounds with
molecular weights above the molecular weight cutoff are retained in
the retentate, and the compounds with molecular weights below the
cutoff pass through the filter into the permeate. Ultrafiltration
methods typically are not capable of removing low molecular weight
organic compounds and ions.
[0028] Ultrafiltration is typically a cross-flow separation
process. The liquid stream to be treated (feed) flows tangentially
along the membrane surface, separating into one stream that passes
through the membrane (permeate) and another that does not
(retentate or concentrate). The operating parameters of the
ultrafiltration system can be varied to achieve the desired result.
For example, the feed mixture to be filtered can be brought into
contact with the membrane by way of applied pressure. The rate of
permeation across the membrane is directly proportional to the
applied pressure; however, the maximum pressure may be limited. The
flow velocity of the mixture across the membrane surface can be
adjusted. Temperature can also be varied. Typically, permeation
rates increase with increasing temperature.
[0029] Commercial ultrafiltration systems are readily available and
may be used for the ultrafiltration methods of the present
invention. For example, commercial suppliers such as Millipore,
Spectrum.RTM. Labs, Pall Corporation, Whatman.RTM., Porex
Corporation, and Snyder Filtration manufacture various filter
membranes and cartridges, and/or filtration systems (e.g.,
tangential flow filtration systems). Exemplary membranes include,
but are not limited to, Biomax.RTM. and Ultracel.RTM. membranes and
Pellicon.RTM. XL cassettes (from Millipore), Microkros.RTM.,
Minikros.RTM., and KrosFlo.RTM. Hollow Fiber Modules (from
Spectrum.RTM. Labs), and Microza filters and Centramate,.TM.
Centrasette,.TM. Maximate.TM., and Maxisette.TM. Tangential Flow
Filtration Membrane Cassettes. Commercially available filtration
systems include, but are not limited to, Millipore's Labscale.TM.
Tangential Flow Filtration (TFF) system and Spectrum.RTM. Labs'
KrosFlo.RTM. and MiniKros.RTM. Tangential Flow Filtration
Systems.
[0030] Filters and/or membranes that may be useful according to the
present invention include those with molecular weight cutoffs of
less than about 100,000 Da, less than about 75,000 Da, less than
about 50,000, less than about 25,000 Da, less than about 20,000 Da,
less than about 15,000 Da, less than about 10,000 Da, and less than
about 5,000 Da. In certain embodiments, a multistage filtration
process is used to provide an extract with improved clarity. Such
embodiments employ multiple filters and/or membranes of different
(typically decreasing) molecular weight cutoffs. Any number of
filters and/or membranes can be used in succession according to the
invention. For example, a first filtration may be conducted using a
50,000 Da molecular weight cutoff filter and a second filtration
may be conducted using a 5,000 Da molecular weight cutoff
filter.
[0031] According to the present invention, the ultrafiltration
process is designed to achieve a tobacco extract having a decreased
level of suspended solids, and thus an increased level of clarity.
For example, depending on the molecular weight cutoff of the
filters, the ultrafiltered extract may comprise only compounds with
molecular weights below about 50,000, below about 25,000, below
about 10,000 Da, below about 7,500 Da, below about 5,000 Da, below
about 2,500 Da, or below about 1,000 Da. The ultrafiltered extract
typically comprises primarily sugars, nicotine, and amino
acids.
[0032] The ultrafiltered extract exhibits a level of improvement in
clarity over the non-ultrafiltered extract. Clarity of the extract,
and tobacco products according to the invention made therefrom, is
typically defined in terms of translucency. As used herein,
"translucent" or "translucency" refers to materials allowing some
level of light to travel therethrough diffusely. In certain
embodiments, certain materials of the invention (e.g., certain
tobacco extracts or final smokeless tobacco products made
therefrom) can have such a high degree of clarity that the material
can be classified as "transparent" or exhibiting "transparency,"
which is defined as a material allowing light to pass freely
through without significant diffusion. The clarity of the
ultrafiltered extract is such that there is some level of
translucency as opposed to opacity (which refers to materials that
are impenetrable by light).
[0033] The improvement in clarity of the ultrafiltered extract over
the non-ultrafiltered extract can be quantified by any known
method. For example, optical methods such as turbidimetry (or
nephelometry) and colorimetry may be used to quantify the
cloudiness (light scattering) and the color (light absorption),
respectively, of the ultrafiltered extract or products made
therefrom. Translucency can also be confirmed by visual inspection
by simply holding the material (e.g., extract) or product up to a
light source and determining if light travels through the material
or product in a diffuse manner.
[0034] In certain embodiments, the ultrafiltered extract is
analyzed by contacting the extract with light and measuring the
percent of light that has not been absorbed and/or dispersed by the
extract. The measurement can be done, for example, using a standard
spectrophotometer at a given wavelength. The spectrophotometer is
typically calibrated with deionized water, which is assigned a
transparency value of 100%. Acceptable levels of
translucency/transparency at a given wavelength in the
ultrafiltered extract can vary. Typically, the ultrafiltered
extract has a translucency of greater than about 5%, greater than
about 10%, greater than about 15%, greater than about 20%, greater
than about 25%, greater than about 30%, greater than about 40%,
greater than about 50%, greater than about 60%, greater than about
60%, greater than about 70%, greater than about 80%, or greater
than about 90%. Typically, the ultrafiltered extract will not be
colorless, and will have some discernible brown/black coloring.
Following ultrafiltration, the extract can be stored in the
refrigerator or freezer or the extract can be freeze dried or spray
dried prior to use in the products of the invention. In certain
embodiments, it is provided in syrup form.
[0035] Although in some embodiments, the tobacco extract is used
directly, it may be desirable to heat treat the extract. This
thermal treatment can be conducted before the ultrafiltration,
after the ultrafiltration, or both before and after the
ultrafiltration. For example, a tobacco material can be thermally
processed by mixing the tobacco material, water, and an additive
selected from the group consisting of lysine, glycine, histidine,
alanine, methionine, glutamic acid, aspartic acid, proline,
phenylalanine, valine, arginine, di- and trivalent cations,
asparaginase, saccharides, phenolic compounds, reducing agents,
compounds having a free thiol group, oxidizing agents (e.g.,
hydrogen peroxide), oxidation catalysts, plant extracts, and
combinations thereof, to form a moist tobacco mixture; and heating
the moist tobacco mixture at a temperature of at least about
60.degree. C. to form a heat-treated tobacco mixture. In one
embodiment, the treated tobacco extract is heat treated in the
presence of water, NaOH, and an additive (e.g., lysine) at about
88.degree. C. for about 60 minutes. Such heat treatment can help
prevent acrylamide production resulting from reaction of asparagine
with reducing sugars in tobacco materials and can provide some
degree of pasteurization. See, for example, US Pat. Pub. No.
2010/0300463 to Chen et al., which is incorporated herein by
reference. In certain embodiments wherein a heat-treated tobacco
extract is used in a smokeless tobacco product of the present
invention, the product can be characterized by very low acrylamide
content. For example, in some embodiments, the smokeless tobacco
product is characterized by an acrylamide content of less than
about 500 ppb (ng/g), less than about 400 ppb, less than about 300
ppb, less than about 200 ppb, or less than about 100 ppb.
[0036] Accordingly, "treated tobacco extract" as used herein refers
to a tobacco extract that has been treated in some way to remove
high molecular weight components and thereby improve clarity (e.g.,
an ultrafiltered extract). The "treated tobacco extract" may or may
not be heat-treated as described herein.
[0037] The treated tobacco extract is used in the production of
smokeless tobacco products. Accordingly, the present invention
provides translucent or transparent smokeless tobacco products
comprising tobacco-derived material. Exemplary smokeless tobacco
products of the invention have the form of a lozenge, tablet,
microtab, or other tablet-type product. See, for example, the types
of nicotine-containing lozenges, lozenge formulations, lozenge
formats and configurations, lozenge characteristics and techniques
for formulating or manufacturing lozenges set forth in U.S. Pat.
No. 4,967,773 to Shaw; U.S. Pat. No. 5,110,605 to Acharya; U.S.
Pat. No. 5,733,574 to Dam; U.S. Pat. No. 6,280,761 to Santus; U.S.
Pat. No. 6,676,959 to Andersson et al.; U.S. Pat. No. 6,248,760 to
Wilhelmsen; and U.S. Pat. No. 7,374,779; US Pat. Pub. Nos.
2001/0016593 to Wilhelmsen; 2004/0101543 to Liu et al.;
2006/0120974 to Mcneight; 2008/0020050 to Chau et al.; 2009/0081291
to Gin et al.; and 2010/0004294 to Axelsson et al.; which are
incorporated herein by reference. The amount of material contained
within each piece (e.g., each unit of lozenge type of product) can
vary. For example, a representative unit for lozenge products
generally weighs at least about 100 mg, often at least about 200
mg, and frequently at least about 300 mg; while the weight of a
representative unit for such products generally does not exceed
about 1.5 g, often does not exceed about 1 g, and frequently does
not exceed about 0.75 g.
[0038] The amount of treated tobacco extract within the overall
composition can vary. The treated tobacco extract can be provided
in varying concentrations, which can affect the amount of extract
included in the mixture. The amount of extract is at least about
0.5%, generally at least about 1%, often at least about 1.5%, often
at least about 2%, often at least about 2.5%, and frequently at
least about 3% by weight of the product mixture. In certain
embodiments, the amount of extract is at least about 4%, at least
about 5%, at least about 6%, or at least about 7% by weight of the
product mixture. The amount of treated tobacco extract added to the
product mixture is typically not more than about 20%. Exemplary
types of such products can incorporate about 3% by weight, about 4%
by weight, about 4.5% by weight of the mixture, or about 7.5% by
weight of the mixture.
[0039] Although sucrose can be used in the preparation of the
smokeless tobacco products of the present invention, the smokeless
tobacco products are typically sugar-free products, comprising one
or more sugar substitutes. "Sugar-free" as used herein is intended
to include products having less than about 1/15th sugar by weight,
or less than about 1/10th sugar by weight.
[0040] Accordingly, in one embodiment, the smokeless tobacco
product comprises a sugar substitute. The sugar substitute is
typically provided in pure, solid form (e.g., granular or powdered
form). In certain embodiments, the sugar substitute is dry,
comprising a very low water content. For example, the sugar
substitute can comprise less than about 5% water by weight, less
than about 3% water by weight, less than about 2% water by weight,
or less than about 1% water by weight.
[0041] The sugar substitute can be any sugarless material (i.e.,
sucrose-free material) and can be natural or synthetically
produced. The sugar substitute used in the invention can be
nutritive or non-nutritive. For example, the sugar substitute is
commonly a sugar alcohol. Sugar alcohols that may be useful
according to the present invention include, but are not limited to,
erythritol, threitol, arabitol, xylitol, ribotol, mannitol,
sorbitol, dulcitol, iditol, isomalt, maltitol, lactitol,
polyglycitol, and mixtures thereof. For example, in certain
embodiments, the sugar alcohol is selected from the group
consisting of erythritol, sorbitol, and isomalt. The amount of
sugar substitute in the smokeless tobacco product mixture can vary,
but is typically at least about 75%, at least about 80%, at least
about 85%, or at least about 90% by weight of the mixture.
[0042] In certain embodiments, the sugar substitute is capable of
forming a glassy matrix. The formation of a glassy matrix is
commonly characterized by a translucent/transparent appearance.
Typically, the sugar substitute is substantially non-hygroscopic.
Non-hygroscopic materials typically do not absorb, adsorb, and/or
retain a significant quantity of moisture from the air. For
example, in some embodiments, the sugar substitute exhibits a
weight gain of water of less than about 50% upon exposure to
conditions of 25.degree. C., 80% relative humidity for two weeks.
Typically, the sugar substitute exhibits a weight gain of less than
about 30%, less than about 20%, less than about 10%, less than
about 5%, less than about 2%, or less than about 1% upon exposure
to conditions of 25.degree. C., 80% relative humidity for two
weeks. Non-hygroscopic materials can provide the benefit of
reducing the tendency of the smokeless tobacco product to tackify
upon exposure to humidity.
[0043] In certain embodiments, the sugar substitute comprises one
or more sugar alcohols. For example, in one embodiment, the sugar
substitute is isomalt. Isomalt is a disaccharide that is typically
made by enzymatic rearrangement of sucrose into isomaltulose,
followed by hydrogenation to give an equimolar composition of
6-O-.alpha.-D-glucopyranosido-D-sorbitol (1,6-GPS) and
1-O-.alpha.-D-glucopyranosido-D-mannitol-dihydrate
(1,1-GPM-dihydrate).
[0044] In addition to the treated extract and sugar substitute, the
smokeless tobacco product of the present invention contains a
syrup, e.g., a sugar syrup or a sugar alcohol syrup. "Sugar alcohol
syrup" as used herein is intended to refer to a thick solution of
sugar alcohol in water, e.g., having greater than about 40% solids,
preferably having greater than about 50% solids, greater than about
60% solids, greater than about 70% solids, or greater than about
80% solids. Typically, the solid content of the sugar alcohol syrup
primarily comprises the named sugar alcohol (i.e., maltitol syrup
typically comprises greater than about 80%, greater than about 85%,
or greater than about 90% by weight maltitol on a dry basis). Sugar
alcohol syrups are generally prepared by heating a solution of the
sugar alcohol in water and cooling the mixture to give a viscous
composition. The resulting syrup is typically characterized by a
relatively high concentration of sugar alcohol and relatively high
stability (i.e., the sugar alcohol typically does not crystallize
from solution, e.g., at room temperature).
[0045] The syrup, e.g., sugar alcohol syrup, desirably is capable
of affecting the re-crystallization of a melted sugar substitute.
One exemplary sugar alcohol syrup that is particularly useful
according to the present invention is maltitol syrup. Other sugar
alcohol syrups can be used, including, but not limited to, corn
syrup, golden syrup, molasses, xylitol, mannitol, glycerol,
erythritol, threitol, arabitol, ribitol, mannitol, sorbitol,
dulcitol, iditol, isomalt, lactitol, and polyglycitol syrups. Such
sugar alcohol syrups can be prepared or can be obtained from
commercial sources. For example, maltitol syrups are commercially
available from such suppliers as Corn Products Specialty
Ingredients. Although sugar alcohol syrups may be preferred, sugar
syrups can, in certain embodiments, be used in place of or in
combination with the sugar alcohol syrup. For example, in some
embodiments, corn syrup, golden syrup, and/or molasses can be
used.
[0046] The amount of sugar alcohol syrup added to the smokeless
tobacco product mixture is typically that amount required to slow
recrystallization of the sugar substitute in melted form. One of
skill in the art would understand the need to vary the amount of
sugar alcohol syrup depending on the composition of the remaining
ingredients to ensure that the recrystallization is sufficiently
slow to provide a material with the desired characteristics (e.g.,
a desired level of translucency/transparency). Accordingly, the
amount of sugar alcohol syrup can vary, but typically ranges from
about 0.1% to about 2%, often from about 0.5% to about 1.5%, and
more often about 1% by weight of the smokeless tobacco product
mixture. In certain embodiments, the amount of sugar alcohol syrup
is higher, for example, up to about 2% by weight of the mixture, up
to about 5% by weight of the mixture, up to about 10% by weight of
the mixture, or up to about 20% by weight of the mixture
[0047] In certain embodiments, the smokeless tobacco product
further comprises a salt. The presence of a salt in the smokeless
tobacco product may act to suppress bitterness and/or enhance
sweetness. Any type of salt can be used. Common table salt (NaCl)
is typically used according to the present invention, but other
types of salts are intended to be encompassed as well. The amount
of salt added may vary, but typically ranges from 0% to about 8%,
for example from about 1% to about 4% or from about 0% to about 2%,
often around 1% by weight of the smokeless tobacco product. In some
embodiments, a somewhat salty taste is a desirable feature of the
smokeless tobacco product.
[0048] In some embodiments, the composition according to the
invention also contains one or more buffering agents and/or pH
adjusters (i.e., acids or bases). In some embodiments, one or more
buffering agents and/or pH adjusters are added to the mixture to
ensure that the final smokeless tobacco product has a pH within a
desirable range. Exemplary pH ranges in such smokeless tobacco
products are generally from about 6-11, and often about 7-10 (e.g.,
about 7 or about 8). In such embodiments, the amount of buffering
agent and/or pH adjuster added to the smokeless tobacco product
mixture is simply that amount required to bring the formulation to
or keep the formulation at the desired pH. The amount of buffering
agent and/or pH adjuster added to any given formulation can be
readily calculated by one skilled in the art and may comprise, for
example, about 0.5% to about 1% by weight of the mixture. It is
noted that in certain embodiments, a basic pH is not necessary in
the products of the present invention. Accordingly, certain
products of the present invention have a pH of less than about 6 or
less than about 5 (e.g., from about 4 to about 6).
[0049] Various food-grade buffering agents are known and can be
used to adjust the pH of the products of the present invention.
Suitable buffering agents include those selected from the group
consisting of acetates, glycinates, phosphates, glycerophosphates,
citrates such as citrates of alkaline metals, carbonates, hydrogen
carbonates, and borates, and mixtures thereof. In certain
embodiments, the buffering agent is an amino acid, as taught for
example, in US Pat. Pub. No. 2008/0286341 to Andersson et al. and
PCT Appl. No. WO2008/040371 to Andersson et al., which are both
incorporated herein by reference. As noted therein, various amino
acids and salts thereof are useful for this purpose, including, but
not limited to, arginine, asparigine, glutamic acid, glutamine,
glycine, histidine, isoleucine, leucine, lysine, methionine,
phenylalanine, serine, threonine, valine, cysteic acid,
N-glycylglycine, and ornithine. In certain embodiments,
N-glycylglycine or L-lysine is added as a buffering agent. In some
embodiments, an amino acid buffering agent is used in combination
with another amino acid buffering agent and/or in combination with
one or more non-amino acid buffering agents. In certain
embodiments, the optional pH adjusting agent is a base (e.g.,
NaOH). In certain embodiments, L-lysine and NaOH are added to the
compositions of the present invention.
[0050] In some embodiments, one or more additional sweeteners are
added to the compositions of the present invention. The one or more
additional sweeteners can comprise any natural or artificial
sweetener, including, but not limited to, sugar or any of the sugar
substitutes described previously. In certain embodiments, the
sweetener can include, glycyrrhizin, glycerol, inulin, lactitol,
mabinlin, maltitol, mannitol, miraculin, monatin, monellin,
osladin, pentadin, polydextrose, sorbitol, stevia, tagatose,
thaumatin, acesulfame potassium, alitame, aspartame, cyclamate,
dulcin, glucin, neotame, saccharin, sucralose, and combinations
thereof. In certain embodiments, the sweetener comprises sucralose
(1,6-Dichloro-1,6-dideoxy-.beta.-.sub.D-fructofuranosyl-4-chlor-
o-4-deoxy-.alpha.-.sub.D-galactopyranoside). The amount of
sweetener added can vary, but is typically that amount required for
a sufficiently "sweet" taste. For example, sweetener can be added
to make the sweetness of the smokeless tobacco product comparable
to that of sugar. In particular embodiments, sucralose is added in
an amount of about 0.5% to about 2% by weight of the mixture, often
in an amount of about 1% by weight of the mixture.
[0051] Various natural and/or artificial flavorants can also be
added to the smokeless tobacco products of the present invention,
and the character of these flavors can be described as, without
limitation, fresh, sweet, herbal, confectionary, floral, fruity or
spicy. Specific types of flavors include, but are not limited to,
vanilla (e.g., vanillin optionally in complexed form), coffee,
chocolate, cream, mint, spearmint, menthol, peppermint,
wintergreen, lavender, cardamon, nutmeg, cinnamon, clove,
cascarilla, sandalwood, honey, jasmine, ginger, anise, sage,
licorice, lemon, orange, apple, peach, lime, cherry, and
strawberry. See also, Leffingwill et al., Tobacco Flavoring for
Smoking Products, R. J. Reynolds Tobacco Company (1972), which is
incorporated herein by reference. Flavorings also can include
components that are considered moistening, cooling or smoothening
agents, such as eucalyptus. Flavorings can also include sensates,
which can add a range of tactile, organoleptic properties to the
smokeless tobacco products. For example, sensates can provide a
warming, cooling, or tingling sensation. These flavors may be
provided neat (i.e., alone) or in a composite (e.g., spearmint and
menthol, or orange and cinnamon). Flavorants of this type can be
present in an amount of from about 0.5% to about 15%, often between
about 0.5% and about 1.5% by weight of the product mixture. In
certain embodiments, the flavorant is present in any amount of at
least about 0.5% by weight or at least about 0.75% by weight of the
mixture.
[0052] Various other substances can be added to the compositions of
the present invention. For example, excipients such as fillers or
carriers for active ingredients (e.g., calcium polycarbophil,
microcrystalline cellulose, hydroxypropylcellulose, sodium
carboxymethylcellulose, cornstarch, silicon dioxide, calcium
carbonate, lactose, and starches including potato starch, maize
starch, etc.), thickeners, film formers and binders (e.g.,
hydroxypropyl cellulose, hydroxypropyl methylcellulose, acacia,
sodium alginate, xanthan gum and gelatin), antiadherents (e.g.,
talc), glidants (e.g., colloidal silica), humectants (e.g.,
glycerin), preservatives and antioxidants (e.g., sodium benzoate
and ascorbyl palmitate), surfactants (e.g., polysorbate 80), dyes
or pigments (e.g., titanium dioxide or D&C Yellow No. 10), and
lubricants or processing aids (e.g, calcium stearate or magnesium
stearate) are added to the compositions in certain embodiments.
[0053] It is well-known that nicotine is subject to oxidation and
accordingly, it may be advantageous to incorporate one or more
anti-oxidants, such as, e.g., ascorbyl palmitate and/or sodium
ascorbate, in a composition according to the invention. The one or
more anti-oxidants may be present in a concentration of from about
0.05% w/w to about 0.3% w/w, such as, e.g., from about 0.1% w/w to
about 0.25% w/w or from about 0.15% w/w to about 0.2% w/w in the
smokeless tobacco product mixture.
[0054] Certain products of the present invention also can have
outer coatings (e.g., an outer coating can be composed of
ingredients such as carnauba wax and/or pharmaceutically acceptable
forms of shellacs, glazing compositions and surface polish agents).
Application of a coating can be accomplished using techniques such
as airless spraying, fluidized bed coating, use of a coating pan,
or the like. Materials for use as a coating can be polymeric in
nature, such as cellulosic material (e.g., cellulose butyrate
phthalate, hydroxypropyl methylcellulose phthalate, and
carboxymethyl ethylcellulose), and polymers and copolymers of
acrylic acid, methacrylic acid, and esters thereof.
[0055] Representative compositions according to the present
invention can have various types of formats and configurations, and
as a result, the character, nature, behavior, consistency, shape,
form, size and weight of the composition can vary. The shape of a
representative composition can be generally spherical, cylindrical
(e.g., ranging form the general shape of a flattened disc to the
general shape of a relatively long, slender stick), helical,
obloid, square, rectangular, or the like; or the composition can
have the form of a bead, granular powder, crystalline powder,
capsule, film, strip, gel, or the like. The shape of the
composition can resemble a wide variety of pill, tablet, lozenge,
capsule, and caplet types of products.
[0056] The manners and methods used to formulate and manufacture
the smokeless tobacco product can vary. For example, the
compositions can be prepared via any method commonly used for the
preparation of hard boiled confections. Exemplary methods for the
preparation of hard confections can be found, for example, in LFRA
Ingredients Handbook, Sweeteners, Janet M. Dalzell, Ed.,
Leatherhead Food RA (Dec. 1996), pp. 21-44, which is incorporated
herein by reference.
[0057] Typically, a first mixture of ingredients is prepared. The
composition of the first mixture of ingredients can vary; however,
it typically comprises a sugar substitute and may contain various
additional substances (e.g., the sugar alcohol syrup, NaCl,
preservatives, further sweeteners, water, and/or flavorings). In
certain embodiments, it comprises the sugar substitute, salt, and
vanillin. In other embodiments, the first mixture comprises the
sugar substitute and the sugar alcohol syrup. Typically, the first
mixture of ingredients does not contain the treated tobacco extract
or other tobacco material.
[0058] The first mixture of ingredients is heated until it melts;
subsequently, the mixture is heated to or past the hard crack
stage. In confectionary making, the hard crack stage is defined as
the temperature at which threads of the heated mixture (obtained by
pulling a sample of cooled syrup between the thumb and forefinger)
are brittle or as the temperature at which trying to mold the syrup
results in cracking. According to the present method, the
temperature at which the hard crack stage is achieved can vary,
depending on the specific makeup of the product mixture but
generally is between about 145.degree. C. and about 170.degree. C.
Typically, the mixture is not heated above about 171.degree. C.,
which is the temperature at which caramelization begins to occur.
In the processes of the present invention, the mixture is typically
heated to the hard crack stage temperature or above and then
allowed to cool. The heating can be conducted at atmospheric
pressure or under vacuum. Typically, the method of the present
invention is conducted at atmospheric pressure.
[0059] In one exemplary embodiment, the first mixture of
ingredients comprises a high percentage of isomalt and the mixture
is heated to about 143.degree. C. Once all components are
dissolved, the temperature is raised past the hard crack stage
(e.g., to about 166.degree. C.). The mixture is heated to this
temperature and then removed from the heat to allow the mixture to
cool.
[0060] In certain embodiments, the treated tobacco extract and,
optionally, additional components (e.g., additional sweeteners,
fillers, flavorants, and water) as described above are separately
combined. The treated tobacco extract-containing mixture is added
to the first mixture of ingredients, typically after the first
mixture of ingredients has been removed from the heat. The addition
of the treated tobacco extract-containing mixture may, in some
embodiments, occur only after the heated first mixture of
ingredients has cooled to a predetermined temperature (e.g., in
certain embodiments, to about 132.degree. C.). In certain
embodiments, one or more flavorants are added to the treated
tobacco extract-containing mixture immediately prior to adding the
mixture to the first, heated mixture of ingredients. Certain
flavorants are volatile and are thus preferably added after the
mixture has cooled somewhat.
[0061] The combined mixture is then formed into the desired shape.
In certain embodiments, the mixture is poured directly into molds,
formed (e.g., rolled or pressed) into the desired shape, or
extruded. If desired, the mixture can be extruded or injection
molded. In certain embodiments, the mixture is formed or extruded
into a mold of desired shape in an enclosed system, which may
require decreased temperature and which may limit evaporation of
certain mixture components. For example, such a system may limit
the evaporation of volatile components including, but not limited
to, flavorants. Other methods of producing smokeless tobacco
products and/or lozenges are also intended to be encompassed
herein.
[0062] Although the foregoing description has focused on treated
tobacco extract-containing smokeless tobacco products, it is noted
that the compositions and methods are intended to encompass other
tobacco-derived or non-tobacco derived smokeless tobacco products
as well. For example, tobacco-derived or non-tobacco derived
nicotine or a derivative thereof can be used in place of the
treated tobacco extract. As mentioned above, nicotine may be
present in any suitable form. Normally, nicotine is selected from
the group consisting of nicotine base, nicotine hydrochloride,
nicotine dihydrochloride, nicotine monotartrate, nicotine
bitartrate, nicotine sulfate, nicotine zinc chloride such as
nicotine zinc chloride monohydrate and nicotine salicylate. In some
embodiments, nicotine is in its free base form, which can
optionally be sorbed on a carrier (e.g., microcrystalline
cellulose) for inclusion in a smokeless tobacco product. See, for
example, the nicotine/carrier compositions set forth in US Pat.
Pub. No. 2004/0191322 to Hansson, which is incorporated by
reference herein.
[0063] Typical conditions associated with manufacture of food grade
products such as described herein include control of heat and
temperature (i.e., the degree of heat to which the various
ingredients are exposed during manufacture and the temperature of
the manufacturing environment), moisture content (e.g., the degree
of moisture present within individual ingredients and within the
final composition), humidity within the manufacturing environment,
atmospheric control (e.g., nitrogen atmosphere), airflow
experienced by the various ingredients during the manufacturing
process, and other similar types of factors. Additionally, various
process steps involved in product manufacture can involve selection
of certain solvents and processing aids, use of heat and radiation,
refrigeration and cryogenic conditions, ingredient mixing rates,
and the like. The manufacturing conditions also can be controlled
due to selection of the form of various ingredients (e.g., solid,
liquid, or gas), particle size or crystalline nature of ingredients
of solid form, concentration of ingredients in liquid form, or the
like. Ingredients can be processed into the desired composition by
techniques such as extrusion, compression, spraying, and the
like.
[0064] In certain embodiments, the smokeless tobacco product is
transparent or translucent as defined herein.
Transparency/translucency can be determined by any means commonly
used in the art; however, it is commonly measured by
spectrophotometric light transmission over a range of wavelengths
(e.g., from about 400-700 nm). Transmission measurements for the
smokeless tobacco products of the present invention are typically
higher than those of traditional tobacco-extract containing
smokeless tobacco products. Translucency can also be confirmed by
visual inspection by simply holding the smokeless tobacco product
up to a light source and determining if light travels through the
product in a diffuse manner.
[0065] Aspects of the present invention are more fully illustrated
by the following examples, which are set forth to illustrate
certain aspects of the present invention and are not to be
construed as limiting thereof.
EXPERIMENTAL
Ultrafiltration of Tobacco Extract
[0066] A tobacco extract is prepared by mixing hot water
(140-155.degree. C.) and tobacco at a ratio of 8:1 water:tobacco.
The mixture is agitated for 1 hour and is then centrifuged. The
supernatant thus obtained is evaporated to .about.25% solids. The
extract is centrifuged again (4000 rpm for 10 min) in 50 mL conical
tubes to remove any large particles that remain. The supernatant is
filtered using a vacuum filter system and 7 .mu.m filter paper.
[0067] The filtered supernatant is diluted 1:1 with distilled,
deionized water and placed in the reservoir of a Millipore
Tangential Flow Filter (TFF) system. A first TFF system was fitted
with a Pellicon Biomax-50 (MWCO 50,000 Da) cartridge. A second TFF
system was fitted with a Pellicon Biomax-5 (MWCO 5,000 Da)
cartridge. The permeate passing through the first TFF system is
directed into the reservoir of the second TFF system. The resulting
final permeate is collected in a clean beaker. This ultrafiltered
extract is placed in a freezer at -80.degree. C. overnight, and
then removed and placed in a freeze drier. The tray of the freeze
drier was set to -20.degree. C. and the vacuum was set at 0.600
mBar. The extract is kept in the freeze drier until dry,
approximately 36-48 hours.
[0068] Beginning with 600 mL of evaporated tobacco extract
(.about.25% solids), 50 g of freeze-dried material was obtained.
Assuming 60% of the water was evaporated from the initial tobacco
material, the extract represented 1500 mL (1500 g) of water that
was exposed to 187.5 g tobacco (8:1 water:tobacco ratio). Of that
mass, 45% (84.4 g) is hot water extractable. Of the hot water
extractable material, 59% passed through the ultrafiltration
freeze-drying process (i.e., 26.6% of the starting tobacco mass
made it through the ultrafiltration freeze-drying process).
[0069] The ultrafiltered, freeze-dried extract has the consistency
of light brown sugar, is highly hygroscopic, and has a
pleasant/sweet aroma. Analysis shows that the extract contains
sugars, organic acids, salts, alkaloids, and nicotine. In humid
conditions, it forms a brown, viscous, translucent syrup. The
ultrafiltered, freeze-dried extract has much less color and more
clarity than the initial tobacco extract.
Preparation of Smokeless Tobacco Product (With No Heat
Treatment)
[0070] Isomalt, NaCl, and vanillin are mixed in a pot and the
temperature of the mixture is brought to 143.degree. C. The mixture
is held at 143.degree. C. until the isomalt is melted and the
temperature is then increased to 166.degree. C. In a separate
vessel, treated tobacco extract, maltitol syrup, H.sub.2O,
sucralose, and, optionally, L-lysine are mixed to form a solution.
Optionally, in a second separate vessel, water and sodium hydroxide
are mixed to form a solution.
[0071] The isomalt mixture is removed from the heat and allowed to
cool to 132.degree. C. The remaining components (i.e., the extract
containing solution and optional sodium hydroxide solution) are
combined and, optionally, one or more flavorings are added to the
combined solution. The combined solution is poured into the hot
isomalt mixture and folded in.
[0072] The resulting mixture is poured into molds to form smokeless
tobacco products. When the mixture becomes too viscous to pour, the
mixture can be heated in a microwave using high heat (e.g., for
about 7 seconds). Representative smokeless tobacco product mixtures
are set forth below. Mixture 1 below contains no base, while
Mixtures 2 and 3 contain sodium hydroxide at varying levels.
TABLE-US-00001 MIXTURE 1 Ingredient Percent by weight Isomalt ST-M*
90.37 Maltitol syrup 1.00 Ultrafiltered tobacco extract (77%
solids) 3.84 NaCl 1.00 Vanillin 0.30 Sucralose 0.20 H.sub.2O 3.16
Flavorant 0.13 Final pH = 4.5 *Isomalt in which 1,6-GPS and 1,1-GPM
are present in essentially equimolar amounts and which has a medium
grain size, the diameter of approximately 90% of all particles
being <3 mm.
TABLE-US-00002 MIXTURE 2 Ingredient Percent by weight Isomalt ST-M
90.37 Maltitol syrup 1.00 Ultrafiltered tobacco extract (77%
solids) 3.84 NaCl 1.00 Vanillin 0.30 Sucralose 0.20 H.sub.2O 3.01
Flavorant 0.13 NaOH 0.15 Final pH = 6.6
TABLE-US-00003 MIXTURE 3 Ingredient Percent by weight Isomalt ST-M
90.37 Maltitol syrup 1.00 Ultrafiltered tobacco extract (77%
solids) 3.84 NaCl 1.00 Vanillin 0.30 Sucralose 0.20 H.sub.2O 2.86
Flavorant 0.13 NaOH 0.30 Final pH = 8.1
Preparation of Smokeless Tobacco Product (With Heat-Treated Tobacco
Extract)
[0073] Certain smokeless tobacco products are prepared using
tobacco extract that has been heat treated with different additives
to reduce the amount of acrylamide. A heat-treated tobacco extract
is prepared by combining an ultrafiltered tobacco extract with an
additive to reduce acrylamide in water and stirring until a
solution is formed. The resulting mixture is heated to 88.degree.
C. and held at this temperature for 60 minutes. The mixture is
cooled and additional water is added to return the mixture to the
starting weight of 200 g.
[0074] Mixtures 4-7, described in the tables below, relate to
smokeless tobacco products comprising heat-treated tobacco extract
prepared in this way. Part A outlines the components of the heat
treatment process. The mixtures comprise different additives for
the reduction of acrylamide. The resulting heat-treated tobacco
extract can be stored frozen until use. This heat-treated tobacco
extract is used in the preparation of a smokeless tobacco product
according to the method provided above, using the components
detailed in Part B of Mixtures 4-7.
[0075] As one specific example, heat-treated tobacco extract is
prepared by combining H.sub.2O (65.79 g), treated tobacco extract,
77% solids (118.42 g), NaOH (8.90 g), and L-lysine (6.89 g),
stirring until dissolved, heating to 88.degree. C., and holding at
this temperature for 60 minutes. The mixture is cooled to
29.degree. C. and additional H.sub.2O is added to return the
mixture to the starting weight of 200 g.
TABLE-US-00004 MIXTURE 4 Part A - Extract Treatment with NaOH and
L-lysine Ingredient Grams Ultrafiltered tobacco extract (77%
solids) 118.42 H.sub.2O 65.79 NaOH 8.50 L-lysine 7.29 Part B -
Preparation of Smokeless Tobacco Product Ingredient Percent by
weight Isomalt ST-M 90.00 Maltitol syrup 1.00 Heat-treated tobacco
extract 7.60 NaCl 1.00 Vanillin 0.10 Sucralose 0.15 Flavorant 0.15
Final pH = 7.76
TABLE-US-00005 MIXTURE 5 Part A - Extract Treatment with NaOH and
L-cysteine 97% Ingredient Grams Ultrafiltered tobacco extract (77%
solids) 118.42 H.sub.2O 65.79 NaOH 8.50 L-cysteine 97% 7.29 Part B
- Preparation of Smokeless Tobacco Product Ingredient Percent by
weight Isomalt ST-M 90.00 Maltitol syrup 1.00 Heat-treated tobacco
extract 7.60 NaCl 1.00 Vanillin 0.10 Sucralose 0.15 Flavorant 0.15
Final pH = 7.86
TABLE-US-00006 MIXTURE 6 Part A - Extract Treatment with NaOH and
Asparaginase Ingredient Grains Ultrafiltered tobacco extract (77%
solids) 118.42 H.sub.2O 65.79 NaOH 8.50 Asparaginase 1.50 Part B -
Preparation of Smokeless Tobacco Product Ingredient Percent by
weight Isomalt ST-M 90.00 Maltitol syrup 1.00 Heat-treated tobacco
extract 7.60 NaCl 1.00 Vanillin 0.10 Sucralose 0.15 Flavorant 0.15
Final pH = 8.29
TABLE-US-00007 MIXTURE 7 Part A - Extract Treatment with NaOH and
3% Hydrogen Peroxide Ingredient Grams Ultrafiltered tobacco extract
(77% solids) 118.42 NaOH 50% solution 17.00 3% hydrogen peroxide
solution 80.00 Part B - Preparation of Smokeless Tobacco Product
Ingredient Percent by weight Isomalt ST-M 90.00 Maltitol syrup 1.00
Heat-treated tobacco extract 7.60 NaCl 1.00 Vanillin 0.10 Sucralose
0.15 Flavorant 0.15 Final pH = 8.10
[0076] The compositions comprising heat-treated tobacco extract
exhibited relatively low acrylamide levels in the final smokeless
tobacco products (Mixture 4=343 ng/g, Mixture 5=44.8 ng/g, Mixture
6=190 ng/g, and Mixture 7=445 ng/g). These acrylamide levels
represent a significant decrease as compared with tobacco extract
that has not been heat treated. For example, heat treated tobacco
extract can exhibit up to about a 98% reduction in acrylamide level
over non-heat-treated tobacco extract. The values for smokeless
tobacco products represented by Mixtures 4-7 represent a reduction
in acrylamide level of from about 60% to about 96% over a
comparable smokeless tobacco product wherein the tobacco extract
has not been heat treated.
[0077] Many modifications and other embodiments of the invention
will come to mind to one skilled in the art to which this invention
pertains having the benefit of the teachings presented in the
foregoing description. Therefore, it is to be understood that the
invention is not to be limited to the specific embodiments
disclosed and that modifications and other embodiments are intended
to be included within the scope of the appended claims.
[0078] Although specific terms are employed herein, they are used
in a generic and descriptive sense only and not for purposes of
limitation.
* * * * *